Process of removing oil from mineral-oil-sulphonic bodies



Patented @ct. :11; I929 CHARLES FISCHER, JR., AND WARREN T. REDD-ISH, OF CINCINNATI, OHIO, ASSIGNORS TO THE TWITCHELL PROCESS COMPANY,' OF CINCINNATI, OHIO, A. CORPORATION OF OHIO PROCESS OF REMOVING OIL FROM MINERAL-OIL-SULPHONIC BODIES No Drawing. Application filed June 29,

Our invention relates to a process of separating oil and sulphonated components thereof.

The oils embraced within the scope of this invention are those hydrocarbon oils characterized by the presence of certain components susceptible to modification by the action of sulphuric acid and certain components not susceptible. Oils such; as petroleum, shale oil and coal tar oil', gilsonitic distillates and many other fractions 01'' distillates of hydrocarbon deposits usually exemplify this characteristic.

Since petroleum is commercially available at present in large quantities, the following disclosure is made in relation thereto.

l/Vhen petroleum or fractions thereof, such as lubricating stock, are treated with sulphuric acid, certain components of the oil are modified. The theory chemically accepted at present explains this modification as sulphonation, i. e. the sulphuric acid reacts with components of the mineral oil (the unsaturated components, supposedly) to form mineral oil sulphonic acid. The yield ofv sulphonic acid is higher when the oil is treated with fuming sulphuric acid, so this disclosure is also made in relation to this fuming sulphuric acid treatment.

It is further theory that these mineral oil sulphonic acids can be reacted with metallic substance or compounds such as sodium hydroxide or sodium carbonate, for instance, to produce salts of mineral oil sulphonic acid. Research to date seems to indicate that these assumptions are correct, but in the ensuing description of the invention and the claims, it is to be understood that the procedure and products thereof as described is the real substance of the invention and that the chemical explanation is merely offered for the benefit of the skilled in the art.

This above described sulphonating treatment is practiced on a large commerclal scale in the refining of medicinal white oil. In this refining operation the sulphonated components are the by-products and are commercially available as such at present.

These sulphonated components are usually" available in the form of alkaline salts since 1926. Serial No. 119,483.

the sulphonated components in the acid state have a highly corrosive actionpn iron or steel pipes or containers. The advantage of treating, shipping or handling these sulphonated 1,286,179 to Robert E. I-Iumphries, issued November 26, 1918.

The sulphonic bodies commercially available as a result of the practice of the above specified processes are-known as com-inercially pure. These processes do not 0 'mpletely separate all of the oil from the sulphonated components. In fact, the oil and sulphonated components are so intimately mixed, so closely associated and/or possessed of such physical affinity for each other that complete or even approximately complete removal of all the oil has not heretofore been practical.

Therefore one objectof our invention is to provide a process of separating oil and sulphonated components thereof.

Another object of our invention is to provide a process of removing oil from the mineral oil-sulphonates available as a result of the practice of the Petroif, Humphries and other known commercial processes.

In commercial practice a mineral oil fraction such as a lubricating stock is treated with fumin sulphuric acid. Two layers are formed. T eupper layer is known as the A layer and the lower layer as the B layer. The A layer containing sulphonic acids known as mahogany acids is removed and treated with dilute aqueous alcohol and sodium carbonate.

Again two layers are formed. The upper layer is known as the oil layer and the lower layer known as the alkaline alcoholic sublye. The lower layer contains sodium sulphonates known in the art as mahogany soap. The layers are parted and the aqueous alcohol is distilled from the lower layer leaving the maof the vacuum type is recommended, though atmospheric stills can be used.

In treating a mahogany soap such as is produced as above described, the soap is first dehydrated by heating it to a temperature between 100 and 110 C.

The mahogany soap can be dehydrated either in the still, or in any other suitable apparatus. We prefer not to use the still for this purpose as there is considerable foaming during dehydration and therefore there is danger of soap coming over into condensers or catchalls. Also this foaming can be watched and controlled more easil in an opentank than in a still, then, too, d t1on is accomplished faster in an open tank,

for the sides and top of the still would act as a condenser for the water vapors that come from soap, giving reflux action. After the foaming ceases the soap settles, an action which denotes a satisfactory degree of dehydration.

The mahogany soap is then introduced into the still and heated to an oil distilling range of temperature usually between 185 and 230 -C. Super-heated steam of slightly higher temperature, 25 C. for instance, is then introduced through a distributor at the bottom of the still. The steam so introduced serves as an agitator for the soap. The oil is carried off by the steam in vapor phase and can be recovered as a by-product by condensation.

The percentage and amount of oil removed depends upon the length of the treatment and the degree of heat, the amount increasing with each and both.

For instance,if a mahogany soap containing. about 25% oil is dehydrated, then heated to about 200 C. and then agitated with superheated steam at 225 C. for a period of from 6 to 8 hours, all but about 5% of the oil will be removed. The resulting product though not chemically pure provides afar m'ore powerful reagent than the original mahogany soap when both are reconstituted as acids for fat splitting purposes, for instance, in the soap industry.

Thus we provide a process of removing oil from the sulphonated components of the oil in order to render more potent sulphonic reagents commercially available.

Having described our invention, we claim:

1. The process of purifying mahogany sulphonates which comprises dehydrating the sulphonates and agitating the sulphonates with superheated steam to remove in vapor ehydra- 4 our names.

CHARLES FISCHER, JR.

W. T. REDDISH. 

